CN103304222B - Method for combustion-synthesis casting of Al2O3/ZrO2 eutectic ceramic - Google Patents

Method for combustion-synthesis casting of Al2O3/ZrO2 eutectic ceramic Download PDF

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CN103304222B
CN103304222B CN201310213766.3A CN201310213766A CN103304222B CN 103304222 B CN103304222 B CN 103304222B CN 201310213766 A CN201310213766 A CN 201310213766A CN 103304222 B CN103304222 B CN 103304222B
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郑永挺
杨攀
赫晓东
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Harbin Institute of Technology
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Abstract

The invention discloses a method for combustion-synthesis casting of Al2O3/ZrO2 eutectic ceramic, relates to a preparation method of the eutectic ceramic and particularly relates to a method for combustion-synthesis casting of the Al2O3/ZrO2 eutectic ceramic. The invention aims at solving the technical problems that the size of the Al2O3/ZrO2 eutectic ceramic is small and is limited and the temperature in the reaction process is low to cause fewer eutectic structures and bad ceramic performance. The method disclosed by the invention has the advantages that a reaction agent is metal powder and nitrate, a diluting agent is Al2O3 and ZrO2, raw materials are ignited and react by heat released from burning of the metal powder and the nitrate, the reaction temperature can reach 4300K, and is high, and then the raw materials are fully mixed in a liquid phase, so that the number of the eutectic structures is large, the ceramic performance is good, the reaction time is less than 10min, the preparation period is short, the cost is low, and the product purity is high. The method can be applied in the field of preparation of the eutectic ceramic.

Description

A kind of Al 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic
Technical field
The present invention relates to a kind of preparation method of eutectic ceramic, particularly a kind of Al 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic.
Background technology
Al 2o 3/ ZrO 2eutectic ceramic, with its high intensity, good toughness, excellent mechanical behavior under high temperature, thermostability and low crack-sensitivity degree, can be applicable to the material under hot environment or high temperature oxidation stability condition.
The conventional preparation method of eutectic ceramic mainly contains following several: Bridgman method, LASER HEATING Fu Liu district method, micro-daraf(reciprocal of farad), deckle feed embrane method and combustion synthesis method.
The principle of Bridgman method (falling crucible method) is that reactant is put into crucible, then crucible is put into the burner hearth that ruhmkorff coil is housed.By ruhmkorff coil, burner hearth is heated to more than reactant fusing point, allows crucible slowly decline in burner hearth, make the material melting in crucible.Then, along with the decline of crucible, bottom takes the lead in departing from heating zone, after below the fusing point that temperature drops to material, starts crystallization.For different materials, resistance furnace or induction heating can be adopted.The advantage of Bridgman method is: (1) can prepare large-sized block materials; (2) sample with complicated shape can be prepared.Shortcoming has: (1) speed of growth is slow; (2) production cost is higher; (3) thermograde is less, and the spacing of each eutectic phase is comparatively large, the performance of impact tissue.
LASER HEATING Fu Liu district method (also known as LZF method) using laser as thermal source, concentrate by energy height, produces high temperature melting stupalith.Compared with traditional technology of preparing, LASER HEATING method has higher thermograde, can reach (10 4k/cm).The advantage of the method is: thermograde is high, pollution-free, without the need to crucible, fast growth etc.The higher material of fusing point also can rapid melting cooling, and the material structure obtained is comparatively thin, and the performance of material is significantly improved.Different according to the scanning speed of laser, the micromechanism of melting range eutectic structure can be very different, and can control the performance of material whereby.But the impact of Stimulated Light spot diameter, its product size is also restricted.
Micro-daraf(reciprocal of farad) (μ-PD method) is the same with Bridgman method is heat in crucible, and the crucible bottom unlike micro-daraf(reciprocal of farad) has a hole.After the material melts in crucible, melt grows downwards along aperture under crucible.This method can preparation property is identical or interface separation is little tissue, compared with additive method, is more suitable for preparing the less fibrous crystals of diameter.By changing the shape of crucible, eutectic rod or the eutectic fiber of various size can be prepared.The eutectic structure microtexture that this method obtains is better, so have excellent mechanical property, compared with can preparing the Bridgman method of large size eutectic, the intensity of eutectic fiber is higher.But the sample size prepared of the method is too small is also its main drawback.
It is in the crucible that eutectic melt is housed, immerse refractory metal powder type film that deckle feeds embrane method (border epitaxial method), utilizes the wicking action of liquid, and melt rises along the pore in type film.The thermograde on type film surface is 400 ~ 1600K/cm, can obtain the different sample of size according to the difference of pull rate, can continuous production eutectic material.The advantage of the method is: thermograde is large, and the material produced has outstanding mechanical property.Shortcoming is: the sample size of preparation is little, shape is single.
Combustion synthesis method (combustion synthesis), also known as self-propagating high-temperature synthesis (being called for short SHS), is proposed by USSR (Union of Soviet Socialist Republics) scientist Merzhanov.This method is without the need to external heat source, and when being dependence raw material id reaction, liberated heat is to carry out the technology of inorganic refractory synthesis.The advantage of the method is: cost is low, it is low to consume energy, temperature of reaction is high, growth efficiency is high.Shortcoming is: because growth velocity is too high, can cause larger residual thermal stress, final product may be caused to occur fracture phenomena at material internal.
The people such as the current existing Zhao Zhong people are at " conbustion synthesis Al under hypergravity 2o 3/ ZrO 2composition, Structure and Properties " in adopt the method that combines with hypergravity of conbustion synthesis to prepare the Y of large-size 2o 3doped with Al 2o 3/ ZrO 2eutectic ceramic, is of a size of 100*100*15mm 3, relative density is 98.7% to the maximum.Its ultimate principle is: adopt high temperature aluminum thermal response 3Cr 2o 3+ 6Al=3Al 2o 3+ 6Cr, metal-powder chromium in product adopts ultracentrifugal mode to be separated, the output capacity of eutectic ceramic is by restriction to a certain extent, the impact that simultaneous reactions temperature is subject to the boiling temperature of Cr in raw material improves further certain difficulty, the boiling point of Cr is 2945K, if temperature is greater than 2945K, the pressure of system can increase sharply on the one hand, causes the security of preparation technology to reduce; On the other hand because a large amount of heats is taken away in the vaporization of Cr, determine that the temperature of its reaction system is lower, can not be too many more than 2945K, and in rapid cooling system, if temperature is lower, raw material may be caused insufficient in liquid-phase mixing, eutectic structure is few, affects the performance of eutectic ceramic.
Existing one section of title being published in APPLIED SURFACE SCIENCE for 2011 and author are (" Microstructure and mechanism of Al 2o 3-ZrO 2eutectic coating prepared by combustion-assisted thermal explosion spraying " author: Yongting Zheng, Hongbo Li, Tao Zhou) document, adopt detonation flame spraying to prepare Al in the document 2o 3/ ZrO 2eutectic coating, the title separately having a section to be published in JOURNAL OF ALLOYS AND COMPOUNDS for 2012 and author are (" Microstructure and mechanical properties of Al 2o 3/ ZrO 2eutectic ceramic composites prepared by explosion synthesis " author: Yongting Zheng, Hongbo Li, Tao Zhou, Jing Zhao, Pan Yang) document, in the document adopt blast synthesis prepared Al 2o 3/ ZrO 2eutectic ceramic, but aforesaid method all has following shortcoming: and (1) reaction pressure is large, in 30 ~ 100MPa scope, has blast impulse effect simultaneously, and very large (2) Product size of preparation technology's danger is little, is Φ 20*40mm to the maximum 3.
Summary of the invention
The present invention is for solving existing Al 2o 3/ ZrO 2eutectic ceramic size is little, the technical problem that size-constrained system and reaction process temperature lowly cause that ceramic eutectic structure is few, ceramic performance is bad, and provides a kind of Al 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic.
A kind of Al of the present invention 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic is carried out according to the following steps:
One, nitrate is placed on independent drying treatment in loft drier, obtains nitrate reaction agent;
Two, metal-powder is placed on drying treatment in vacuum drying oven, obtains metal-powder reagent; Wherein said metal-powder reagent is the mixture of Al or Al and Ti;
Three, thinner is placed on drying treatment in vacuum drying oven, obtains thinner;
Four, the metal-powder reagent that nitrate reaction agent step one obtained, step 2 obtain and the thinner that step 3 obtains, mixed by ball milling, then load in reaction unit, light raw material, carry out combustion heat release reaction, reaction times < 10min, temperature of reaction < 4300K, reaction pressure < 10MPa, gets rid of the gas in reaction system, obtains Al in reaction process 2o 3/ ZrO 2eutectic ceramic; The mol ratio of metal-powder reagent that wherein the nitrate reaction agent that obtains of the step one described in step 4 and step 2 obtain is 3: (24 ~ 33), and wherein in the step one described in step 4, in nitrate reaction agent and step 2, the ratio of the thinner that the quality sum of metal-powder reagent obtains with step 3 is 1: (1.188 ~ 1.786).
The inventive method reagent is metal-powder and nitrate, and thinner is Al 2o 3and ZrO 2light raw material, reacted by the combustion heat release of metal-powder and nitrate, method of the present invention has the following advantages: (1) by the combustion heat release of metal-powder and nitrate be swift in response all substances in heating systems temperature to system fusing point more than, by strictly controlling the percentage composition of thinner, hierarchy of control temperature remains on more than the fusing point of all substances in system, and this reaction is the controlled combustion reactions of speed; (2) without under centrifugal, high temperature, large-sized condition, get rid of the gas of system by methods such as mechanical shock, ultrasonic vibration or induction stirring, make ceramic dense; (3) under centrifugal condition, setting centrifugal force is 10g ~ 500g, can obtain fully dense as cast condition eutectic structure, through cooling fast, solidifying, and getable large-sized Al 2o 3/ ZrO 2eutectic ceramic, size can reach Φ 500mm; (4) if centrifugal force is little, the Al of (TiN or ZrN) dispersion-strengthened can be obtained 2o 3/ ZrO 2eutectic ceramic, if centrifugal force is large, TiN or ZrN is completely segregated, and obtains Al 2o 3/ ZrO 2eutectic ceramic; (5) add suitably excessive metal-powder reagent, can neutralize nitrogen in the reaction, reaction is carried out under normal pressure or very low pressure, and reaction pressure is 0.1MPa ~ 10MPa, and reaction pressure is low, fully can ensure the security of producing; (6) temperature of reaction can reach 4300K, and temperature of reaction is high, and make raw material abundant in liquid-phase mixing, thus make eutectic structure many, ceramic performance is good; (7) speed of synthesis process is controlled, but compared to traditional technology synthesis rapidly, efficiency is high, reaction times, with the production size of product, the difference of synthesis technique and changing, is generally 1min ~ 10min, and preparation cycle is short and without the need to external heat source, rely on reaction self-heat generation heating systems, cost is low, and products therefrom purity is high, can be applicable to the preparation field of eutectic ceramic.
Accompanying drawing explanation
Fig. 1 is Al prepared by embodiment 3 2o 3/ ZrO 2the electron scanning micrograph of eutectic ceramic.
Embodiment
Technical scheme of the present invention is not limited to following embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of Al of present embodiment 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic is carried out according to the following steps:
One, nitrate is placed on independent drying treatment in loft drier, obtains nitrate reaction agent;
Two, metal-powder is placed on drying treatment in vacuum drying oven, obtains metal-powder reagent; Wherein said metal-powder reagent is the mixture of Al or Al and Ti;
Three, thinner is placed on drying treatment in vacuum drying oven, obtains thinner;
Four, the metal-powder reagent that nitrate reaction agent step one obtained, step 2 obtain and the thinner that step 3 obtains, mixed by ball milling, then load in reaction unit, light raw material, carry out combustion heat release reaction, reaction times < 10min, temperature of reaction < 4300K, reaction pressure < 10MPa, gets rid of the gas in reaction system, obtains Al in reaction process 2o 3/ ZrO 2eutectic ceramic; The mol ratio of metal-powder reagent that wherein the nitrate reaction agent that obtains of the step one described in step 4 and step 2 obtain is 3: (24 ~ 33), and wherein in the step one described in step 4, in nitrate reaction agent and step 2, the ratio of the thinner that the quality sum of metal-powder reagent obtains with step 3 is 1: (1.188 ~ 1.786).
The reactional equation of present embodiment is as follows:
33Al+3Zr(NO 3) 4→12Al 2O 3+3ZrN+9AlN (1)
8Al+Al(NO 3) 3→3Al 2O 3+3AlN (2)
Or (1) (2) mixing between the two
20Al+12Ti+3Zr(NO 3) 4→10Al 2O 3+3ZrO 2+12TiN (3)
5Al+3Ti+Al(NO 3) 3→3Al 2O 3+3TiN (4)
Or (3) (4) mixing between the two
Wherein equation (1) (2) (3) (4) at high temperature have follow-up reaction as follows:
4AlN+3ZrO 2→3ZrN+2Al 2O 3+0.5N 2
2Al+N2→2AlN
2Ti+N2→2TiN
The method reagent of present embodiment is metal-powder and nitrate, and thinner is Al 2o 3and ZrO 2light raw material, reacted by the combustion heat release of metal-powder and nitrate, the method of present embodiment has the following advantages: (1) is swift in response more than heating systems temperature to the fusing point of all substances by the combustion heat release of metal-powder and nitrate, by strictly controlling the percentage composition of thinner, hierarchy of control temperature remains on more than the fusing point of all substances in system, and this reaction is the controlled combustion reactions of speed; (2) without under centrifugal, high temperature, large-sized condition, get rid of the gas of system by methods such as mechanical shock, ultrasonic vibration or induction stirring, make ceramic dense; (3) under centrifugal condition, setting centrifugal force is 10g ~ 500g, has obtained fully dense as cast condition eutectic structure, simultaneously through cooling fast, solidifying, and getable large-sized Al 2o 3/ ZrO 2eutectic ceramic, size can reach Φ 500mm; (4) if centrifugal force is little, the Al of (TiN or ZrN) dispersion-strengthened can be obtained 2o 3/ ZrO 2eutectic ceramic, if centrifugal force is large, TiN or ZrN is completely segregated, and obtains Al 2o 3/ ZrO 2eutectic ceramic; (5) add excessive metal-powder reagent, can nitrogen be neutralized in the reaction, reduce the pore in product, reaction is carried out under normal pressure or very low pressure, reaction pressure is 0.1MPa ~ 10MPa, and reaction pressure is low, fully can ensure the security of producing; (6) temperature of reaction can reach 4300K, and temperature of reaction is high, and make raw material abundant in liquid-phase mixing, thus make eutectic structure many, ceramic performance is good; (7) speed of synthesis process is controlled, but compared to traditional technology synthesis rapidly, efficiency is high, reaction times is with the production size of product, the difference of synthesis technique and changing, be generally 1min ~ 10min, preparation cycle is short and cost is low, and products therefrom purity is high, can be applicable to the preparation field of eutectic ceramic.
Embodiment two: present embodiment and embodiment one unlike: the nitrate reaction agent described in step one is Zr (NO 3) 4with Al (NO 3) 3in one or both mixture.Other step and parameter identical with embodiment one.
When nitrate reaction agent in present embodiment is mixture, both are with arbitrarily than mixing.
Embodiment three: under one of present embodiment and embodiment one to two are the condition by temperature being 50 ~ 70 DEG C unlike: the drying treatment described in step one, time of drying is that 8h ~ 12h realizes.Other step and parameter identical with one of embodiment one to two.
Embodiment four: one of present embodiment and embodiment one to three unlike: when the metal-powder reagent described in step 2 is the mixture of Al and Ti, the mol ratio of Al with Ti is that 5: 3 other steps and parameter are identical with one of embodiment one to three.
Embodiment five: under one of present embodiment and embodiment one to four are the condition by temperature being 70 ~ 90 DEG C unlike: the drying treatment described in step 2, time of drying is that 8h ~ 12h realizes.Other step and parameter identical with one of embodiment one to four.
Embodiment six: under one of present embodiment and embodiment one to five are the condition by temperature being 70 ~ 90 DEG C unlike: the drying treatment described in step 3, time of drying is that 8h ~ 12h realizes.Other step and parameter identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: the thinner described in step 3 is by Al 2o 3and ZrO 2composition, and the Al after reaction in system 2o 3and ZrO 2meet eutectic ratio.Other step and parameter identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: described thinner is by Al 2o 3, ZrO 2with stablizer composition, and the Al after reaction in system 2o 3and ZrO 2meet eutectic ratio, described Al 2o 3and ZrO 2quality sum and the mass ratio of stablizer be 1: (0.031 ~ 0.147), wherein said stablizer is yttrium oxide or magnesium oxide.Other step and parameter identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike: the ball milling described in step 4 is by under ball material mass ratio is the condition of 3: 1, ball milling mixing 4h ~ 6h realize.Other step and parameter identical with one of embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: in step 4, temperature of reaction is 2300K ~ 4300K, and in step 4, reaction pressure is 0.1MPa ~ 10MPa.Other step and parameter identical with one of embodiment one to nine.
Embodiment 11: one of present embodiment and embodiment one to ten are by without under centrifugal condition unlike: the gas got rid of in the reaction process described in step 4 in reaction system, adopt mechanical shock, ultrasonic vibration or induction stirring to realize.Other step and parameter identical with one of embodiment one to ten.
Embodiment 12: one of present embodiment and embodiment one to ten one unlike: the gas got rid of in the reaction process described in step 4 in reaction system is by under centrifugal condition, be arranged on by reaction unit in centrifugation systems, setting centrifugal force is that 10g ~ 500g realizes; Described centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.Other step and parameter identical with one of embodiment one to ten one.
With following verification experimental verification beneficial effect of the present invention:
Embodiment 1, a kind of Al 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic is carried out according to the following steps:
One, by Zr (NO 3) 45H 2o is placed in loft drier dry separately, and drying temperature is 60 DEG C, and time of drying is 10h, obtains Zr (NO 3) 4;
Two, be placed on by Al and Ti in vacuum drying oven dry, drying temperature is 80 DEG C, and time of drying is 10h;
Three, by Al 2o 3and ZrO 2be placed in vacuum drying oven dry, drying temperature is 80 DEG C, and time of drying is 10h;
Four, the Zr (NO that 61.8g step one obtains is taken 3) 4, the Al that obtains of Ti, 84.5g step 3 of obtaining of Al, 34.9g step 2 of obtaining of 32.8g step 2 2o 3with the ZrO that 86.0g step 3 obtains 2by ball milling mixing 5h, ball material mass ratio is 3: 1, then loads in reaction unit, reaction unit is arranged in centrifugation systems, setting centrifugal force is 10g, then lights raw material, carries out combustion heat release reaction, reaction times is 10min, temperature of reaction is 3300K, and reaction pressure is 2MPa, obtains the Al that scantling is the TiN dispersion-strengthened of Φ 100mm 2o 3/ ZrO 2eutectic ceramic; Wherein said centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.
Embodiment 2, a kind of Al 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic is carried out according to the following steps:
One, by Zr (NO 3) 45H 2o is placed in loft drier dry separately, and drying temperature is 60 DEG C, and time of drying is 10h, obtains Zr (NO 3) 4;
Two, be placed on by Al in vacuum drying oven dry, drying temperature is 80 DEG C, and time of drying is 10h;
Three, by Al 2o 3and ZrO 2be placed in vacuum drying oven dry, drying temperature is 80 DEG C, and time of drying is 10h;
Four, the Zr (NO that 62.4g step one obtains is taken 3) 4, the Al that obtains of Al, 37.5g step 3 of obtaining of 52.9g step 2 2o 3with the ZrO that 147.2g step 3 obtains 2by ball milling mixing 5h, ball material mass ratio is 3: 1, then loads in pressure-resistant reaction device, pressure-resistant reaction device is arranged in centrifugation systems, setting centrifugal force is 10g, then lights raw material, carries out combustion heat release reaction, reaction times is 10min, temperature of reaction is 3500K, and reaction pressure is 3MPa, obtains the Al of the ZrN dispersion-strengthened being of a size of Φ 150mm 2o 3/ ZrO 2eutectic ceramic; Wherein said centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.
Embodiment 3, a kind of Al 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic is carried out according to the following steps:
One, by Zr (NO 3) 45H 2o is placed in loft drier dry separately, and drying temperature is 60 DEG C, and time of drying is 10h, obtains Zr (NO 3) 4;
Two, be placed on by Al in vacuum drying oven dry, drying temperature is 80 DEG C, and time of drying is 10h;
Three, by Al 2o 3and ZrO 2be placed in vacuum drying oven dry, drying temperature is 80 DEG C, and time of drying is 10h;
Four, the Zr (NO that 65.4g step one obtains is taken 3) 4, the Al that obtains of Al, 31.1g step 3 of obtaining of 55.4g step 2 2o 3with the ZrO that 148.1g step 3 obtains 2by ball milling mixing 5h, ball material mass ratio is 3: 1, then loads in pressure-resistant reaction device, pressure-resistant reaction device is arranged in centrifugation systems, setting centrifugal force is 200g, then lights raw material, carries out combustion heat release reaction, reaction times is 10min, temperature of reaction is 3700K, and reaction pressure is 4MPa, obtains the Al being of a size of Φ 200mm 2o 3/ ZrO 2eutectic ceramic; Wherein said centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.
With the Al that FEI Flied emission environmental scanning electron microscope (Quanta200F, acceleration voltage is 20KV) is prepared the present embodiment 2o 3/ ZrO 2eutectic ceramic carries out Analysis on Microstructure, and result as shown in Figure 1, as can be seen from the figure obtains Al 2o 3/ ZrO 2eutectic structure.
Embodiment 4, a kind of Al 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic is carried out according to the following steps:
One, by Zr (NO 3) 45H 2o is placed in loft drier dry separately, and drying temperature is 60 DEG C, and time of drying is 10h, obtains Zr (NO 3) 4;
Two, be placed on by Al in vacuum drying oven dry, drying temperature is 80 DEG C, and time of drying is 10h;
Three, by Al 2o 3and ZrO 2be placed in vacuum drying oven dry, drying temperature is 80 DEG C, and time of drying is 10h;
Four, the Zr (NO that 68.3g step one obtains is taken 3) 4, the Al that obtains of Al, 24.7g step 3 of obtaining of 58.0g step 2 2o 3with the ZrO that 149.0g step 3 obtains 2by ball milling mixing 5h, ball material mass ratio is 3: 1, then loads in pressure-resistant reaction device, lights raw material, carry out combustion heat release reaction, reaction times is 10min, and temperature of reaction is 3900K, and reaction pressure is 5MPa, by the gas in mechanical vibration eliminating system, obtain the Al being of a size of Φ 300mm 2o 3/ ZrO 2eutectic ceramic.
Embodiment 5, a kind of Al 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic is carried out according to the following steps:
One, by Zr (NO 3) 45H 2o is placed in loft drier dry separately, and drying temperature is 60 DEG C, and time of drying is 10h, obtains Zr (NO 3) 4;
Two, be placed on by Al in vacuum drying oven dry, drying temperature is 80 DEG C, and time of drying is 10h;
Three, by Y 2o 3, Al 2o 3and ZrO 2be placed in vacuum drying oven dry, drying temperature is 80 DEG C, and time of drying is 10h;
Four, the Zr (NO that 65.4g step one obtains is taken 3) 4, the Y that obtains of Al, 6g step 3 of obtaining of 55.4g step 2 2o 3, the Al that obtains of 31.1g step 3 2o 3with the ZrO that 148.1g step 3 obtains 2by ball milling mixing 5h, ball material mass ratio is 3: 1, then loads in pressure-resistant reaction device, pressure-resistant reaction device is arranged in centrifugation systems, setting centrifugal force is 200g, then lights raw material, carries out combustion heat release reaction, reaction times is 10min, temperature of reaction is 3700K, and reaction pressure is 4MPa, obtains the Al being of a size of Φ 200mm 2o 3/ YSZ eutectic ceramic; Wherein said centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.

Claims (4)

1. an Al 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic, is characterized in that a kind of Al 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic is carried out according to the following steps:
One, nitrate is placed on independent drying treatment in loft drier, obtains nitrate reaction agent;
Two, metal-powder is placed on drying treatment in vacuum drying oven, obtains metal-powder reagent; Wherein said metal-powder reagent is Al;
Three, thinner is placed on drying treatment in vacuum drying oven, obtains thinner;
Four, the metal-powder reagent that nitrate reaction agent step one obtained, step 2 obtain and the thinner that step 3 obtains, mixed by ball milling, then load in reaction unit, light raw material, carry out combustion heat release reaction, reaction times <10min, temperature of reaction is 2300K ~ 4300K, reaction pressure is 0.1MPa ~ 10MPa, gets rid of the gas in reaction system, obtain Al in reaction process 2o 3/ ZrO 2eutectic ceramic; The mol ratio of metal-powder reagent that wherein the nitrate reaction agent that obtains of the step one described in step 4 and step 2 obtain is 3:(24 ~ 33), wherein in the step one described in step 4, in nitrate reaction agent and step 2, the ratio of the thinner that the quality sum of metal-powder reagent obtains with step 3 is 1:(1.188 ~ 1.786);
Nitrate reaction agent described in step one is Zr (NO 3) 4with Al (NO 3) 3in one or both mixture;
Drying treatment described in step one is under the condition by being 50 ~ 70 DEG C in temperature, and time of drying is that 8h ~ 12h realizes;
Described thinner is by Al 2o 3, ZrO 2with stablizer composition, and the Al after reaction in system 2o 3and ZrO 2meet eutectic ratio, described Al 2o 3and ZrO 2quality sum and the mass ratio of stablizer be 1:(0.031 ~ 0.147), wherein said stablizer is yttrium oxide or magnesium oxide.
2. a kind of Al according to claim 1 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic, under it is characterized in that the condition that the drying treatment described in step 2 is by temperature being 70 ~ 90 DEG C, time of drying is that 8h ~ 12h realizes, drying treatment described in step 3 is under the condition by being 70 ~ 90 DEG C in temperature, and time of drying is that 8h ~ 12h realizes.
3. a kind of Al according to claim 1 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic, is characterized in that in the reaction process described in step 4, the gas got rid of in reaction system is by without under centrifugal condition, adopts mechanical shock, ultrasonic vibration or induction stirring to realize.
4. a kind of Al according to claim 1 2o 3/ ZrO 2the method of the conbustion synthesis founding of eutectic ceramic, is characterized in that in the reaction process described in step 4, the gas got rid of in reaction system is by under centrifugal condition, is arranged on reaction unit in centrifugation systems, and setting centrifugal force is that 10g ~ 500g realizes; Described centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.
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